Reaktion #163394

ord-5870a4657db34221a6ebc51719ac160a

Reaktionsgleichung

Cl
hydrochloric acid
[OH-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium hydroxide
CO[Si](OC)(OC)c1ccccc1
phenyltrimethoxysilane
CCO[Si](OCC)(OCC)OCC
tetraethoxysilane
CCO[Si](C)(OCC)OCC
methyltriethoxysilane
CO[Si](CCCC1CC(=O)OC1=O)(OC)OC
trimethoxysilylpropyl succinic anhydride
CO[Si](CCCOCC1CO1)(OC)OC
glycidoxypropyltrimethoxysilane
CCOCC(C)O
propylene glycol monoethyl ether
Cl
hydrochloric acid
O=C([O-])CCC(=O)[O-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1.c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium succinic acid salt

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONto be dissolved
  2. 2
    workup.ADDITIONthe resultant mixed solution
  3. 3
    Temperaturwas warmed
  4. 4
    Temperaturto reflux
  5. 5
    Sonstigethe resultant reaction solution
  6. 6
    workup.DISTILLATIONwere distilled off under reduced pressure
  7. 7
    Sonstigeto obtain a hydrolysis-condensation product

Vorschrift

4.81 g of phenyltrimethoxysilane, 70.74 g of tetraethoxysilane, 17.21 g of methyltriethoxysilane, 0.14 g of trimethoxysilylpropyl succinic anhydride, 5.73 g of glycidoxypropyltrimethoxysilane, and 150 g of acetone were charged into a 500 ml flask to be dissolved and the resultant mixed solution was warmed while stirring the mixed solution with a magnetic stirrer to reflux. Next, 32.33 g of a 0.01 M hydrochloric acid aqueous solution was added to the mixed solution. The reaction was carried out for 240 minutes and then the resultant reaction solution was cooled down to room temperature. Then, 200 g of propylene glycol monoethyl ether was added to the reaction solution, and ethanol, water, and hydrochloric acid being reaction by-products were distilled off under reduced pressure to obtain a hydrolysis-condensation product. To the hydrolysis-condensation product, 1.36 g of a 10% by weight triphenylsulfonium hydroxide aqueous solution was added to obtain a triphenylsulfonium succinic acid salt-containing Si polymer. The obtained polymer corresponded to a polymer having five types of unit structures of Formula (3-34). The molecular weight Mw of the obtained polymer measured by GPC was found to be 2,500 in terms of polystyrene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835093B2uspto-grants-2014_09